Delft University of Technology

Viscoelastic and dry-sliding wear properties of basalt fiber-reinforced composites basedon a surface-modified graphene oxide/epoxy matrix

Jamali, N.; Khosravi, H.; Rezvani, A.; Tohidlou, E.; Poulis, J. A.

DOI10.1177/1528083719850839Publication date2019Document VersionFinal published versionPublished inJournal of Industrial Textiles

Citation (APA)Jamali, N., Khosravi, H., Rezvani, A., Tohidlou, E., & Poulis, J. A. (2019). Viscoelastic and dry-sliding wearproperties of basalt fiber-reinforced composites based on a surface-modified graphene oxide/epoxy matrix.Journal of Industrial Textiles, 50(6), 939-953. https://doi.org/10.1177/1528083719850839

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Article

Viscoelastic and dry-sliding wear propertiesof basalt fiber-reinforcedcomposites based ona surface-modifiedgraphene oxide/epoxymatrix

N Jamali1, H Khosravi2 , A Rezvani1, E Tohidlou2 andJA Poulis3

Abstract

The current study focuses on the development of silanized graphene oxide reinforced

basalt fiber/epoxy composites for enhanced tribological and viscoelastic properties. The

modified-graphene oxide nanoplatelets were characterized using energy-dispersive

X-ray spectroscopy, and Raman analyses. Pin-on-disk wear test and dynamic mechanical

thermal analysis were conducted to determine the tribological and viscoelastic proper-

ties of the fabricated specimens with different silanized-graphene oxide loadings in the

matrix (0–0.5 wt.% at a step of 0.1). The multiscale specimens were fabricated using the

hand lay-up technique. The best silanized-graphene oxide loading for effectively enhan-

cing the tribological properties was found to be 0.4 wt.%, whose wear rate and friction

coefficient were 62% and 44%, respectively lower than those of the neat basalt/epoxy

composite. The examination of the worn surfaces showed the enhanced basalt fiber/

epoxy bonding in graphene oxide-reinforced specimen. From the results of dynamic

mechanical thermal analysis, the specimen filled with 0.4 wt.% silanized-graphene oxide

demonstrated the highest increase of 130% and 13.6�C in the storage modulus and glass

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1Department of Chemistry, University of Sistan and Baluchestan, Zahedan, Iran2Department of Materials Engineering, Faculty of Engineering, University of Sistan and Baluchestan, Zahedan,

Iran3Faculty of Aerospace Engineering, Department of Aerospace Structures and Materials, Group of Structural

Integrity and Composites, Delft University of Technology, Delft, The Netherlands

Corresponding author:

H Khosravi, Department of Materials Engineering, Faculty of Engineering, University of Sistan and Baluchestan,

Zahedan, Iran.

Email: hkhosravi@eng.usb.ac.ir

transition temperature as compared to the neat composite. This study indicated that

the addition of silanized-graphene oxide considerably enhanced the tribological and

viscoelastic properties of the fibrous composites.

Keywords

Polymer matrix composites, basalt fiber, graphene oxide, dry-sliding wear, viscoelastic

properties

Introduction

Fiber-reinforced polymers (FRPs) have found vast applications in aerospace, auto-mobile, marine, and defense industries due to their excellent combinations of highstrength-to-weight and modulus-to-weight ratios, superior corrosion resistance, highchemical resistance, and easiness of fabrication [1,2]. Recently, basalt fiber as anenvironmentally friendly material has emerged as a favorable candidate for use asa reinforcing material in FRPs. It has a high strength-to-weight ratio, high thermalresistance, excellent chemical stability, and good corrosion resistance. Additionally,basalt fiber is non-toxic. For these reasons, many attempts have been made to inves-tigate the various properties of basalt fiber-reinforced composites [3–5].

Mechanical behaviors of graphene oxide- (GO) reinforced FRPs have beeninvestigated by several investigators, and they reported that the addition of GOenhances the mechanical properties [6,7]. GO consists of oxidized one-atom-thickgraphene sheets, and its surface is decorated with oxygen-containing groups such ashydroxyl, epoxy and carbonyl groups, making it an excellent choice for high-performance polymer nanocomposites [8–10]. The properties of graphene-basednanocomposites depend deeply on the homogeneous dispersion of the graphenewithin the polymeric matrix as well as the strong interfacial interaction between thegraphene and matrix [11]. The GO nanosheets tend to agglomerate due to van derWaals interactions. In this regard, surface modification is a good strategy to over-come this problem. Among the various routes for the surface modification ofnanofillers, silanization is a very effective method [12,13]. Silane coupling agentswith a typical general structure of (RO)3SiCH2CH2CH2-X have two types of react-ive groups in their both sides, where RO is a hydrolysable alkoxy group, such asacetoxy, methoxy, or ethoxy, and X is an organofunctional group, such as amino,epoxy, etc. A silane coupling agent with two reactive groups in both sides possessesthe ability to couple two dissimilar materials [14].

In past years, multiscale composites containing both micron and nano-sizedreinforcements have gained wide acceptance for tribological applications [15–19].It has been reported that multiscale composites generally exhibit higher wear resist-ance compared to the neat FRPs. In the work of Osterle et al. [15], enhanced wearproperties of an epoxy matrix composite were obtained by a combination of carbonEbers and silica nanoparticles. Ren et al. [16] studied the effect of graphene additionon the tribological response of Nomex fabric/phenolic composite and found that

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2wt.% graphene-filled specimen showed the best wear resistance. In the work ofGuo et al. [17] who investigated the wear behavior of nano-SiO2/short carbon Eber/epoxy composites, the best tribological properties were related to the specimen with4wt.% SiO2 and 6wt.% carbon Eber. Kim et al. [18] found that the wear resistanceof carbon fiber/epoxy specimen was enhanced by the incorporation of carbonnanotubes. Bobbili and Madhu [19] reported that wear rate (WR) and frictioncoefficient of E-glass-epoxy composite were decreased by the addition of multi-walled carbon nanotubes.

The introduction of nanofillers in the structure of FRPs can affect their visco-elastic properties [20–23]. For example, Menbari et al. [20] observed a remarkableimprovement in the storage modulus and Tg of the epoxy/glass Eber/GO compositecompared to the neat one. Hossain et al. [21] found that storage modulus and Tg ofE-glass/polyester composites were increased by 49.5% and 3�C, respectively, due tothe addition of 0.2wt.% carbon nanofiber in the matrix. The results of Zainuddinet al. [22] work showed that storage modulus and Tg of 0.3wt.% CNTs-NH2-filledE-glass/polyester composite were improved by 72% and 24�C compared to the neatE-glass/polyester specimen. The viscoelastic behavior of modiEed CNT-reinforcedbasalt/epoxy specimens was investigated by Lee et al. [23] They found that silanizedcomposites have greater storage modulus and Tg compared to the unmodiEed andoxidized ones.

To the best of our knowledge, no research work has been reported in the literatureon the tribological and viscoelastic properties of multiscale silanized-GO/basaltfiber/epoxy composites, demonstrating the significance of the present study.Herein, basalt fiber reinforced epoxy composites with various silanized-GO loadingswere fabricated and characterized by DMTA and pin-on-disc wear tests.

Experimental

Materials

KER 828 as a medium viscosity liquid epoxy resin (viscosity at 25�C: 12–14 Pa.s)was provided by Kumho P&B Chemicals, Inc., Korea, and employed in 100:10weight ratio concerning the amine hardener. Basalt satin weave fabric (300 g/m2)was supplied by Basaltex Co., Belgium. GO nanoplatelets (6–10 layers, thickness:3.4–7 nm, diameter: 10–50 mm) were purchased from US Research NanomaterialsInc. The SEM image of as-received GO is shown in Figure 1.

In order to surface modification of GO, a silane coupling agent namely3-glycidoxypropyltrimetoxysilane (3-GPTMS) was purchased from MerckChemical Co., Germany.

Employed approach for GO modification

For preparation of silanized-GO, 500mg GO was incorporated in a 160ml solutionof ethanol/water (95:5, v/v) followed by sonication for 10min. Then, 5ml 3-GPTMS

Jamali et al. 3

was added, and the resultant mixture was refluxed at 80�C for 12 h. The pH wasadjusted to around 4 by HCl-37%. The acidic media not only decrease the self-condensation reactions between the hydrolyzed SiOH groups in silane chains, butalso increase the amount of SiOH formation. The dark suspension was centrifuged,and the obtained powder was washed with ethanol to remove any unreacted cou-pling agent. Finally, the silanized-GO was dried at 80�C for 8 h [24,25].

Composite fabrication

Epoxy resin and a certain amount of silanized-GO (0.1–0.5wt.% at a step of 0.1)were initially mixed using an overhead high-shear mechanical stirrer running at2000 r/min for 20min. Subsequently, the resultant viscous mixture was sonicatedfor 30min (Ultrasonic Homogenizer 400W, 24kHz, TOPSONICS Co.) to obtaina homogeneous dispersion. During the sonication, the mixtures were kept within awater-ice bath to hold the mixture temperature around 30–40�C. After degassing, thehardener was added and mixed for 5min. The hand lay-up technique followed bycold pressing was employed for manufacturing the final multiscale silanized-GO/basalt fiber/epoxy composites. The specimens were cured at room temperature. Toapprove the positive effect of silane modification, the trend mentioned above was alsoemployed for fabricating a multiscale specimen containing 0.4wt.% as-received GO.It should be noted that the volume fraction of basalt fiber in the specimens was 0.48.

DMTA and wear tests

To study the viscoelastic behavior of the specimens, DMTA was performedon a Perkin Elmer Diamond DMA according to the ASTM D4065 standard.

Figure 1. SEM image of GO nanoplatelets. GO: graphene oxide.

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The specimens (50� 10� 1.25mm) were tested from 25�C to 150�C (heating rate:3�C/min) at a frequency of 1 Hz and amplitude of 5 mm. The parameters of storagemodulus and glass transition temperature were extracted to study the viscoelasticresponse of fabricated specimens.

To evaluate the tribological properties of the specimens, a pin-on-disk test(ASTM G99) as the most frequently configuration was conducted under dry slidingcondition. The dimension of the wear test specimens was 30� 30� 5mm. A com-mercially 52,100 steel pin (1.5Cr, 1C, 0.35Mn, 0.25Si, HRC 64) with diameter of5mm and height of 20mm was served as a counter component. The wear test wascarried out at a normal load of 20N, the linear velocity of 0.5m/s, and total slidingdistance of 1000m. Specific WR (calculated from equation (1)) [26] and frictioncoefficient (FC) for each specimen were reported.

WR ¼�m

�:F:Lðmm3=N:mÞ ð1Þ

In equation (1), �m, r, F, and L are specimen mass loss, specimen density,normal load, and total sliding distance, respectively.

Characterization methods

To characterize the silanized-GO, Raman, and EDX analyses were performed. AnEDX analyzer (MIRA3TESCAN-XMU) was used to evaluate the elemental ana-lysis of silanized-GO. A Teksan (model: Tekram) Raman spectrometer with laserexcitation of 532 nm was also used to characterize the powders.

The worn surfaces of the specimens were evaluated by a scanning electronmicroscopy (SEM-KYKY 3900 EM), with the aim of obtaining some informationabout the dominant wear mechanisms.

Results and discussion

Characterization of GO and silanized-GO

Raman spectroscopy is known as a powerful technique for characterizing thegraphene nanoplatelets. The Raman spectra of GO and silanized-GO are presentedin Figure 2. Both GO and silanized-GO represents two typical broad bands: D-band (�1350 cm�1) and G-band (�1600 cm�1). The ID/IG is used as a measure ofdisordering density in the GO structure [9]. The ID/IG ratio for GO is 0.879 andafter silanization, this value has increased to 0.912. These results prove the absenceof a significant increase in the number of defects in the GO structure after silaniza-tion with 3-GPTMS.

EDX spectrum of silanized-GO is illustrated in Figure 3. The existence of siliconatom originating from the silane compound in the EDX spectrum of silanized-GOconfirmed that the 3-GPTMS molecules are present on the surface of GO.

Jamali et al. 5

DMTA results

The DMTA test was used to evaluate the effect of silanized-GO at various loadingson the viscoelastic properties of basalt fiber/epoxy composites. Figures 4 to 6 showthe variations of storage modulus (E’), loss modulus (E’’), and loss factor (tan d)with temperature for various multiscale specimens. From Figure 4, the storagemodulus proportionally increases from 0 to 0.4wt.% silanized-GO loading(130% increase at 25�C). This behavior can be explained regarding effective inter-action between the silanized-GO and epoxy matrix resulted from their enormoussurface areas and chemical interactions [12,13]. The improved interfacial inter-action decreases the mobility of the epoxy matrix around the GO and increasesthe specimen stiffness. On the other hand, the storage modulus decreases when thesilanized-GO loading increases from 0.4wt.% to 0.5wt.% (39% decrease). It seems

Figure 3. EDX analysis of silanized-GO. GO: graphene oxide. EDX: energy-dispersive X-ray.

Figure 2. Raman spectra of (a) GO, and (b) silanized-GO. GO: graphene oxide.

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that an increase in density and size of GO agglomerates facilities the molecularmotion and movement of chains, resulting in decreased storage modulus. Besides,due to the higher molecular motion in the rubbery region, a slight influence on thisregion is observed after the incorporation of silanized-GO.

Loss modulus describes the viscosity and relates to the energy used to deformthe material. As can be seen in Figure 5, the peak height of loss modulus for themultiscale specimens shows an increase in comparison to the neat one. The dis-persed GO dissipates energy due to its resistance against viscoelastic deformationof the surrounding matrix. The peak height at 0.5wt.% silanized-GO shows asignificant decrease. The decreased loss modulus at higher nanofiller contents canbe interpreted by increased susceptibility of agglomeration, leading to less energydissipating in the system under viscoelastic deformation.

Figure 5. The loss modulus versus temperature for the multiscale composites with various

silanized-GO loadings. GO: graphene oxide.

Figure 4. The storage modulus versus temperature for the multiscale composites with various

silanized-GO loadings. GO: graphene oxide.

Jamali et al. 7

The glass transition temperature (Tg) is determined by the peak position of lossfactor (tan d) [20,22]. From Figure 6, it can be seen that the loss factor increaseswith an increase in the temperature in the transition region; it maximizes in Tg

following by a continuous decrease in the rubbery region. Multiscale specimensshow higher Tg values compared to the neat specimen. Tg shifts from 67.5�C for theneat specimen to 80.9�C for the 0.4wt.% GO-filled specimen (i.e. 13.4�C increase).This behavior can be interpreted by this fact that the silanized-GO tends to limitthe mobility of the matrix chains through interfacial interactions. At 0.5wt.%silanized-GO, the formation of micro-agglomerates creates stress concentrationregions and reduces the value of Tg (see Figure 11). The height of tan d peakdecreases by the incorporation of silanized-GO due to this reason that the presenceof nanofiller in the matrix prevents the molecular movement. This demonstratesthat the mechanical loss to overcome the friction between the molecular chainsreduces after the GO incorporation.

Wear test results

Figure 9 displays the variations in the friction coefficient (FC) with the slidingdistance for the specimens containing various amounts of silanized-GO. Forcomparison, the values of mean FC for different specimens were extracted fromFigure 7. Figure 8 shows the variation of the mean FC with weight percentages ofthe silanized-GO loading. According to the results, the greatest decrease in the FCis 44% which occurs at 0.4wt.% silanized-GO. During the wear test, frictional heatfocuses around the contact region and as a result, the specimen can easily deform.The addition of silanized-GO, due to its high thermal conductivity, most effectivelydissipates the heat, resulting in a decreased FC. Moreover, for the specimens withsilanized-GO addition, due to the formation of a continuous transfer film on thesurface of steel pin, the values of mean FC decrease (see Figure 11).

Figure 6. The tan d versus temperature for the multiscale composites with various silanized-

GO loadings. GO: graphene oxide.

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Figure 7. Variation in the FC with the sliding distance for the specimens containing various

amounts of silanized-GO. GO: graphene oxide; FC: friction coefficient.

Figure 8. Variation in the mean FC with the silanized-GO loading. GO: graphene oxide; FC:

friction coefficient.

Jamali et al. 9

Figure 9 shows the variation of the WR as a function of silanized-GO loading.Similar to the FC, the WR also decreased with increasing the silanized-GO loadingup to 0.4wt.%, and then the WR increased for the 0.5wt.%. Based on the results,the specimen containing 0.4wt.% silanized-GO gives the best wear resistanceamong the fabricated specimens. At 0.4wt.% silanized-GO, over 62% reductionof WR is observed. This behavior is in agreement with the results of Ren et al. [16]who reported that the addition of functional graphene as a Eller into Nomex fabric/phenolic composite enhanced the tribological properties of the final composite. Thereduction in the WR with the addition of silanized-GO is probably due to thesuperior fiber-matrix interfacial bonding. This can be explained by the followingmechanisms: (i) the GO nano-sheet acts as an interlocking component between thefibers and polymeric matrix; (ii) the mismatch of coefficient of thermal expansion(CTE) between the fiber and polymeric matrix creates high residual stresses duringthe curing stage, resulting in stress concentrations at interface [27]. With the add-ition of silanized-GO, the difference in the CTE of the matrix and fiber reduces.Consequently, the fiber-matrix interfacial bonding enhances [28]. As mentionedbefore, the addition of silanized-GO can effectively dissipate the concentrated fric-tional heat around the contact region, and as a result, the WR decreases.

As observed in Figures 8 and 9, there is a considerable enhancement in the FCand WR for the specimen Elled with 0.5wt.% silanized-GO compared with thespecimen Elled with 0.4wt.% silanized-GO. This may be ascribed to the fact that athigher nanofiller loading, agglomeration of silanized-GO will occur. During thewear condition, these aggregates act as stress-concentration zones and reduce thewear resistance of the specimen.

Figure 10 shows the SEM micrographs from the worn surface of the specimensafter being slid against the 52,100 pin. For the neat specimen (Figure 10(a)), thematrix and fibers are damaged more severely compared to the multiscale speci-mens. Also, poor adhesion of the matrix to the fibers is observable on the wornsurface of the neat specimen. On the contrary, the multiscale specimens

Figure 9. Variation in the WR with the silanized-GO loading. GO: graphene oxide; WR:

wear rate.

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demonstrate an enhanced fiber-matrix bonding. Silanized-GO loading up to0.4wt.% caused enhancement in the interfacial bonding (Figure 10(b) to (e)).However, for the 0.5wt.% GO-loaded specimen, fiber/matrix debonding, matrixcracking and fiber breakage on the worn surface can be observed due to theagglomeration of nano-sheets (Figure 11).

Figure 10. SEM micrographs from the worn surface of the specimens with various silanized-GO

loadings: (a) 0 wt.%, (b) 0.1 wt.%, (c) 0.2 wt.%, (d) 0.3 wt.%, (e) 0.4 wt.%, and (f) 0.5 wt.%; after

being slid against the 52,100 pin. GO: graphene oxide.

Jamali et al. 11

Figure 12. SEM micrographs of the worn 52,100 steel pin against the (a) neat specimen, and

(b) 0.4 wt.% GO-loaded specimen. GO: graphene oxide.

Figure 11. Formation of silanized-GO agglomerates on the surface of 0.5 wt.% GO-loaded

specimen. GO: graphene oxide.

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SEM micrographs of the worn 52,100 steel pin against the neat, and 0.4wt.%GO-loaded specimens are shown in Figure 12. As seen in Figure 12(a), forthe neat specimen, a non-continuous transfer film is formed on the surface ofsteel pin, while a continuous transfer film is observable for the 0.4wt.%GO-loaded specimen (Figure 12(b)). The presence of a continuous transfer filmcan help to diminish the friction by reducing the direct contact between the steel pinand specimen.

Conclusions

In the present study, GO nanoplatelets were surface-modified with 3-glycidoxypro-pyltrimetoxysilane (3-GPTMS). Then, the effect of silanized-GO at various load-ings on the viscoelastic and dry-sliding wear properties of basalt fiber/epoxycomposite was investigated. Based on the experimental results, the following con-clusions were obtained:

1. Results obtained from Raman, and EDX measurements clearly showed that thesilane compound grafted on the GO nanoplatelets successfully.

2. Adding 0.4wt.% of silanized-GO increased the storage modulus and glass tran-sition temperature by 130% and 13.6�C as compared with the neat basalt fiber/epoxy composite.

3. When Elled with 0.4wt.% silanized-GO, the WR and friction coefficient (FC) ofthe multiscale composite are signiEcantly enhanced by 62%, and 44%, respect-ively, compared to the neat basalt fiber/epoxy one.

4. SEM observations from the worn surfaces demonstrated the improvement in thebasalt fiber/epoxy interfacial bonding in the case of the silanized-GO-loadedspecimens.

Acknowledgements

We would like to thank Mrs. Amirabadi, and Dr. Monshi for their cooperation in this work.

Declaration of conflicting interests

The author(s) declared no potential conflicts of interest with respect to the research, author-

ship, and/or publication of this article.

Funding

The author(s) received no financial support for the research, authorship, and/or publicationof this article.

ORCID iD

H Khosravi https://orcid.org/0000-0002-0217-8342E Tohidlou https://orcid.org/0000-0003-2862-7633

Jamali et al. 13

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